Ammonium Chloride → HCID 178420853、化合物

HRID 437592ノート

反応式

HRID 437592 の反応式
[CH:1]1[CH:5]=[C:4]([S:6][CH2:7][C:8]#[N:9])[S:3][CH:2]=1.[N-:10]=[N+:11]=[N-:12].[Na+].[Cl-].[NH4+].[Cl-].[Li+]>CN(C)C=O>[S:3]1[CH:2]=[CH:1][CH:5]=[C:4]1[S:6][CH2:7][C:8]1[NH:12][N:11]=[N:10][N:9]=1

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 433294Lithium ChlorideHCID 21429205(2-Thienylthio)acetonitrile

生成物 1

HCID 178420853HCID 178420853、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 7.76 g. (50 millimoles) of thiophene-2-thioacetonitrile, 4.30 g. (66 millimoles) of sodium azide, 3.55 g. (66 millimoles) of ammonium chloride, and 0.38 g. (9 millimoles) of lithium chloride is maintained for 5 hours at 120° in 50 ml. of dry dimethylformamide. The dimethylformamide is withdrawn under vacuum, the residue is combined with 500 ml. of cold 0.2 N sodium hydroxide solution and extracted with ether. The aqueous phase is adjusted to pH 3 and extracted three times with respectively 150 ml. of ether. The ether phase yields, after drying (Na2SO4) and concentration, the crude, solid tetrazole which is recrystallized once from acetonitrile/water and once from ethanol/water.

後処理

  1. additionA mixture of 7.76 g
  2. customThe dimethylformamide is withdrawn under vacuum
  3. extractionof cold 0.2 N sodium hydroxide solution and extracted with ether
  4. extractionextracted three times with respectively 150 ml
  5. customThe ether phase yields
  6. customafter drying
  7. concentration(Na2SO4) and concentration
  8. customthe crude, solid tetrazole which is recrystallized once from acetonitrile/water and once from ethanol/water

出典と根拠

ORDレコード
ord-bb604464a8444790a08ece4b8de05e57
出典データセット
uspto-grants-1977_06
特許番号
US04031236

反応ノート

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